CN105330985B - A kind of salt bath vulcanization technique of ethylene propylene diene rubber foaming section bar - Google Patents
A kind of salt bath vulcanization technique of ethylene propylene diene rubber foaming section bar Download PDFInfo
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- CN105330985B CN105330985B CN201510771799.9A CN201510771799A CN105330985B CN 105330985 B CN105330985 B CN 105330985B CN 201510771799 A CN201510771799 A CN 201510771799A CN 105330985 B CN105330985 B CN 105330985B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0012—Combinations of extrusion moulding with other shaping operations combined with shaping by internal pressure generated in the material, e.g. foaming
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/16—Ethene-propene or ethene-propene-diene copolymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Physics & Mathematics (AREA)
- Oral & Maxillofacial Surgery (AREA)
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Abstract
The present invention relates to a kind of elastomeric material production technology, more particularly to a kind of salt bath vulcanization technique of ethylene propylene diene rubber foaming section bar.A kind of salt bath vulcanization technique of ethylene propylene diene rubber foaming section bar, the technique include the following steps：After taking foaming raw material mechanical mixture, extruded machine extrusion molding, after salt bath sulfur foam, is made ethylene propylene diene rubber foaming section bar；The foaming raw material includes ethylene propylene diene rubber, naphthenic oil, carbon black, calcium carbonate, stearic acid, zinc oxide, sulphur, accelerating agent dialkyl dithiocarbamate, azodicarbonamide.Present invention employs extrusion molding salt bath vulcanization continuous production processes, production cost is reduced, improves production efficiency.
Description
Technical field
The present invention relates to a kind of elastomeric material production technology, more particularly to a kind of salt bath of ethylene propylene diene rubber foaming section bar
Sulfuration process.
Background technology
For the relatively common dense rubber material of rubber expanded material, common feature most typically is that density is small, light weight,
Specific area is big, and energy absorption capability is strong, and damping, sound insulation and heat-proof quality are good, the series of advantages such as both artistic and practical, in work
The fields such as industry, agricultural, building, communications and transportation, military project, aerospace, daily necessities have been widely used.Such as it is used to seal,
Many occasions such as insulation, vibrationproof anticollision, sound insulation.Huge work is played in scientific and technical research and the development of the national economy
With, it has also become indispensable material during people produce and live.
Ethylene propylene diene rubber（EPDM）It is the rubber formed by the copolymerization of ethene, propylene and a small amount of Third monomer, it
It is made of on main chain chemically stable saturated hydrocarbons, only contains unsaturated double-bond in the side chain, intramolecular is nonpolarity substituent, molecule
Cohesive energy is low, and molecule segment keeps flexible within the scope of wider temperature.Thus there is excellent chemical stability, it is ageing-resistant
Property, chemical proofing, electrical insulating property, impact elasticity and cryogenic property, and hot water resistance can wait.For this reason, EPDM is in rubber
Be more and more widely used in Products Industry, be mainly used for auto parts, electrical apparatus product, industrial product, construction material and
Many aspects such as household supplies and plastic modifier, its expanded material be then widely used in manufacture automobile weather strip, cushion rubber bumper,
The product such as architectural engineering gasket seal, heat-insulating material, damping material, easy diving dress and the footwear of light current component.
Current country EPDM foamed profiles be all added using presulfurization-technique (two step die pressings) of secondary vulcanization produces, but
The length of product is smaller and is unable to continuous production, is to meet that the temperature of presulfurization and sulfur foam, volume will in production process
Ask, need repeatedly more mold exchange, production cycle to need half an hour, production efficiency is very low, and middle more mold exchange can cause to make
The change of product temperature degree, influences the quality of final rubber pange plate.Only Italy, Japan and other countries are proposed rubber in the world
Foaming plate foaming vulcanization tinuous production, but price is very expensive, and maintenance cost is very high.Although EPDM foamed profile performances
It is excellent, but due to production cost and production efficiency etc. reason, limit its industrialized production.Using salt bath vulcanization-foaming work
Skill, the EPDM foamed profile uniform in foaming of preparation, forms hole-closing structure, thermal insulation and sound-proofing are good, and length is larger, speed of production
It is very high, be conducive to it in industries such as building heat preservation, auto parts machinery, waterproof material, electric wire, air conditioner refrigerating, military project apparatuses
Application.
The content of the invention
The defects of present invention is directed to the prior art, there is provided a kind of salt bath vulcanization technique of ethylene propylene diene rubber foaming section bar,
The technique realizes the continuous production of ethylene propylene diene rubber foaming section bar, shortens the production time.
The technical solution adopted by the present invention to solve the technical problems is：
A kind of salt bath vulcanization technique of ethylene propylene diene rubber foaming section bar, the technique include the following steps：Take foaming raw material
After mechanical mixture, extruded machine extrusion molding, after salt bath sulfur foam, is made ethylene propylene diene rubber foaming section bar；Described
Foaming raw material includes ethylene propylene diene rubber, naphthenic oil, carbon black, calcium carbonate, stearic acid, zinc oxide, sulphur, accelerating agent dialkyl group two
Thiocarbamate, azodicarbonamide.
Plasticate 3 minutes preferably, ethylene propylene diene rubber is put on double roll mill, be separately added into naphthenic oil, carbon black,
Calcium carbonate, stearic acid, zinc oxide are kneaded 10 minutes, add sulphur, accelerating agent dialkyl dithiocarbamate, AC mixing
Uniformly, blanking obtains ethylene propylene diene rubber pre-composition after thin logical 10 times；Then ethylene propylene diene rubber pre-composition is squeezed through single screw rod again
Go out machine extrusion molding, under the action of dragger after salt bath sulfur foam, ethylene propylene diene rubber foaming section bar is made.
Preferably, the foaming raw material is made of the component of following parts by weight：100 parts of ethylene propylene diene rubbers, 10 ~ 50
Part naphthenic oil, 5 ~ 40 parts of carbon blacks, 5 ~ 30 parts of calcium carbonate, 0.5 ~ 3.0 part of stearic acid, 1.0 ~ 5.0 parts of zinc oxide, 2.0 ~ 8.0 parts of sulphur
Sulphur, 1.0 ~ 5.0 parts of accelerating agent dialkyl dithiocarbamates, 1.0 ~ 5.0 parts of azodicarbonamides（AC）.
Preferably, the accelerating agent dialkyl dithiocarbamate is selected from zinc dimethyl dithiocarbamate
（PZ）, zinc diethyl dithiocarbamate（ZDEC）, zinc dibutyl dithiocarbamate（BZ）, two thio ammonia of ethylphenyl
Base zinc formate（PX）.
Preferably, each section of temperature control of the single screw extrusion machine, at 50~110 DEG C, wherein feeding section temperature is 50
~60 DEG C, die temperature is 90~110 DEG C.
Preferably, the temperature control of fused salt is at 180~220 DEG C in the salt bath, stop of the material in salt bath
Time is 3 ~ 8 minutes.
Compared with prior art, beneficial effects of the present invention are embodied in following several respects：
1st, ethylene propylene diene rubber foaming section bar produced by the present invention, vulcanization-foaming system used are sulphur/dialkyl group two
Thiocarbamate/azodicarbonamide, wherein vulcanizing agent are sulphur, and accelerating agent is dialkyl dithiocarbamate,
Foaming agent is azodicarbonamide, and accelerating agent dialkyl dithiocarbamate not only accelerates the vulcanization of ethylene propylene diene rubber,
And cause azodicarbonamide activation to reduce its decomposition temperature, the decomposition rate of azodicarbonamide is improved, makes EPDM
The vulcanization of rubber and foaming process form good matching；
2nd, present invention employs salt bath vulcanization foam process, the section bar uniform in foaming of preparation to form hole-closing structure, and size is steady
It is qualitative good；
3rd, present invention employs extrusion molding-salt bath vulcanization continuous production processes, production cost is reduced, improves production
Efficiency.
Embodiment
Below by specific embodiment, technical scheme is described in further detail.It should be appreciated that this hair
Bright implementation is not limited to the following examples, the accommodation in any form of makeing the present invention and/or changes all fall
Enter the scope of the present invention.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments, is the normal of this area unless otherwise instructed
Rule method.
Embodiment 1
100 parts of ethylene propylene diene rubbers are put on double roll mill and are plasticated 3 minutes, 50 parts of naphthenic oils, 40 parts of carbon blacks, 5 parts
Calcium carbonate, 0.5 part of stearic acid, 1.0 parts of zinc oxide are kneaded 10 minutes, add 8.0 parts of sulphur, 5.0 parts of accelerating agent PZ, 5.0 parts
AC is uniformly mixed, and bottom sheet after thin logical 10 times, is made ethylene propylene diene rubber pre-composition, then ethylene propylene diene rubber pre-composition is again through list
Each section of temperature control of screw extruder extrusion molding, wherein single screw extrusion machine is at 50~110 DEG C, and wherein feeding section temperature is 50
~60 DEG C, die temperature is 90~110 DEG C, through 180 DEG C of salt bath sulfur foams 8 minutes under the action of dragger, is made three
First EP rubbers foamed profile.
Embodiment 2
The preparation manipulation of ethylene propylene diene rubber foaming section bar is the same as embodiment 1.The formula of ethylene propylene diene rubber foaming section bar is
100 parts of ethylene propylene diene rubbers, 10 parts of naphthenic oils, 5 parts of carbon blacks, 30 parts of calcium carbonate, 3.0 parts of stearic acids, 5.0 parts of zinc oxide, 2.0 parts
Sulphur, 1.0 parts of ZDEC, 1.0 parts of AC, the temperature of fused salt is 220 DEG C in salt bath, and the salt bath vulcanization time is 3 minutes.
Embodiment 3
The preparation manipulation of ethylene propylene diene rubber foaming section bar is the same as embodiment 1.The formula of ethylene propylene diene rubber foaming section bar is
100 parts of ethylene propylene diene rubbers, 20 parts of naphthenic oils, 15 parts of carbon blacks, 20 parts of calcium carbonate, 2.0 parts of stearic acids, 2.0 parts of zinc oxide, 6.0
Part sulphur, 3.0 parts of BZ, 2.0 parts of AC, the temperature of fused salt is 200 DEG C in salt bath, and the salt bath vulcanization time is 5 minutes.
Embodiment 4
The preparation manipulation of ethylene propylene diene rubber foaming section bar is the same as embodiment 1.The formula of ethylene propylene diene rubber foaming section bar is
100 parts of ethylene propylene diene rubbers, 30 parts of naphthenic oils, 30 parts of carbon blacks, 10 parts of calcium carbonate, 3.0 parts of stearic acids, 3.0 parts of zinc oxide, 6.0
Part sulphur, 4.0 parts of PX, 4.0 parts of AC, the temperature of fused salt is 190 DEG C in salt bath, and the salt bath vulcanization time is 6 minutes.
As a comparison, accelerating agent PZ is by two sulphur of equal parts in the ethylene propylene diene rubber foaming section bar formula of embodiment 1
Change tetra methylthiuram（TMTD）Instead of sulfur foam is carried out in vulcanization bed, curing temperature and time and salt bath vulcanization technique phase
Together, the performance test of gained ethylene propylene diene rubber foaming section bar and production efficiency results contrast are shown in Table 1.
Table 1
| Ethylene propylene diene rubber foaming section bar I | Ethylene propylene diene rubber foaming section bar II | |
| Density（g/cm3） | 0.581 | 0.466 |
| Fracture strength（MPa） | 7.62 | 7.70 |
| Fracture elongation（%） | 544 | 609 |
| Production time（Minute/100 meters） | 115 | 52 |
Ethylene propylene diene rubber foaming section bar I：Be formulated for 100 parts of ethylene propylene diene rubbers, 50 parts of naphthenic oils, 40 parts of carbon blacks, 5 parts
Calcium carbonate, 0.5 part of stearic acid, 1.0 parts of zinc oxide, 8.0 parts of sulphur, 5.0 parts of Vulcanization accelerator TMTDs, 5.0 parts of AC；Ethylene propylene diene rubber
Foamed profile II：Formula and preparation process are the same as by embodiment 6.
From product density as can be seen that comparing sulphur/TMTD/AC, sulphur/dialkyl dithio amino first used is invented
Hydrochlorate/AC effectively improves the expansion ratio of ethylene propylene diene rubber section bar, reduces rubber profile proportion, this is primarily due to dioxane
Zinc ion peripheral electron arrangement in base dithiocar-bamate is 4S24P2With unoccupied orbital, and N, O in blowing agent AC structure
On all have lone pair electrons, according to Louis's Acid-Base be coordinated principle, when the two is combined, on the N, O atom on AC orphan to electricity
Son enters Zn2+Unoccupied orbital, at the same time on the Л keys on-N-C- electron cloud flow ,-N-C- electron cloud concentration is flowed to both sides, in
Between degree of overlapping reduce, thus cause-N-C- keys to be easily broken off, cause AC to activate the reduction of its decomposition temperature.
In terms of mechanical property, the intensity and ductility of ethylene propylene diene rubber foaming section bar prepared by salt bath vulcanization are superior to pass
Material prepared by system vulcanization bed, this is attributable to the cell diameter size of the ethylene propylene diene rubber foaming section bar of salt bath vulcanization preparation
It is smaller, it is distributed than more uniform.From the point of view of production efficiency, ethylene propylene diene rubber foaming is prepared using salt bath vulcanization production technology
The speed of production of section bar is higher than traditional vulcanization bed production technology.
Embodiment described above is a kind of preferable scheme of the present invention, and not the present invention is made in any form
Limitation, also has other variations and remodeling on the premise of without departing from the technical solution described in claim.
Claims (4)
1. a kind of salt bath vulcanization technique of ethylene propylene diene rubber foaming section bar, it is characterised in that the technique includes the following steps：Take
After foaming raw material mechanical mixture, extruded machine extrusion molding, after salt bath sulfur foam, is made ethylene propylene diene rubber foaming type
Material；For the temperature control of fused salt at 180~220 DEG C, material is 3 ~ 8 minutes in the residence time of salt bath in the salt bath；
The foaming raw material is made of the component of following parts by weight：100 parts of ethylene propylene diene rubbers, 10 ~ 50 parts of naphthenic oils, 5 ~ 40 parts of charcoals
Black, 5 ~ 30 parts of calcium carbonate, 0.5 ~ 3.0 part of stearic acid, 1.0 ~ 5.0 parts of zinc oxide, 2.0 ~ 8.0 parts of sulphur, 1.0 ~ 5.0 parts of accelerating agents
Dialkyl dithiocarbamate, 1.0 ~ 5.0 parts of azodicarbonamides（AC）.
2. salt bath vulcanization technique according to claim 1, it is characterised in that：Ethylene propylene diene rubber is put into double roll mill
On plasticate 3 minutes, be separately added into naphthenic oil, carbon black, calcium carbonate, stearic acid, zinc oxide be kneaded 10 minutes, add sulphur, promote
Be uniformly mixed into agent dialkyl dithiocarbamate, AC, after thin logical 10 times blanking obtain ethylene propylene diene rubber pre-composition；So
Ethylene propylene diene rubber pre-composition is again through single screw extrusion machine extrusion molding afterwards, through salt bath sulfur foam under the action of dragger
Afterwards, ethylene propylene diene rubber foaming section bar is made.
3. salt bath vulcanization technique according to claim 1, it is characterised in that：The accelerating agent dialkyl dithio amino
Formates is selected from zinc dimethyl dithiocarbamate（PZ）, zinc diethyl dithiocarbamate（ZDEC）, two sulphur of dibutyl
For carbaminate（BZ）.
4. salt bath vulcanization technique according to claim 2, it is characterised in that：Each section of temperature control of the single screw extrusion machine
System is at 50~110 DEG C, and wherein feeding section temperature is 50~60 DEG C, and die temperature is 90~110 DEG C.
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| CN111875834A (en) * | 2020-06-29 | 2020-11-03 | 桐乡市洲泉振强塑业有限公司 | Foamed rubber anti-collision strip and production process thereof |
| CN113185743B (en) * | 2021-04-30 | 2022-08-09 | 宁波新安东密封保温系统有限公司 | Sealing rubber strip capable of turning directly and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101824189A (en) * | 2010-04-21 | 2010-09-08 | 北京市射线应用研究中心 | Preparation process of ethylene propylene diene rubber foaming materials |
| CN103131091A (en) * | 2013-02-28 | 2013-06-05 | 长城汽车股份有限公司 | Foamed rubber seal strip |
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| CN102690519A (en) * | 2012-06-19 | 2012-09-26 | 西华大学 | Continuous silicon rubber foam plate with low compression stress relaxation and preparation method of continuous silicon rubber foam plate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824189A (en) * | 2010-04-21 | 2010-09-08 | 北京市射线应用研究中心 | Preparation process of ethylene propylene diene rubber foaming materials |
| CN103131091A (en) * | 2013-02-28 | 2013-06-05 | 长城汽车股份有限公司 | Foamed rubber seal strip |
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